• Title/Summary/Keyword: Electrochemical Determination

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The Optimum Conditions for the Simultaneous Determination of Neurotransmitters in Rat Brain Striatum by High Performance Liquid Chromatography with Electrochemical Detection (HPLC-ECD를 이용한 흰쥐 뇌의 선조체 중 신경전달물질의 동시분석시 최적 조건)

  • Kang, Jong-Seong;Mun, Min-Seon;Shin, Hyung-Seon;Lee, Soon-Chul
    • Analytical Science and Technology
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    • v.8 no.2
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    • pp.215-220
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    • 1995
  • A simple, efficient and sensitive method was described for the simultaneous determination of catecholamine, indoleamine and related metabolites from the homogenates of the rat brain striatum by HPLC-ECD. The optimum mobile phase on a reverse phase $C_{18}$ column was 35mM sodium acetate buffer(included 10mM citric acid, 0.13mM $Na_4EDTA$, 0.58mM SOS, pH3-4):MeOH=85:15. The column temperature was $30^{\circ}C$. Dopamine(DA), 3, 4-dihydroxyphenyl acetic acid(DOPAC), homovanilic acid(HVA), 5-hydroxyindole acetic acid(5-HIAA), serotonin(5-HT) and noradrenaline(NA) could be separated and analysed to very small amount. The detection limits of this method were 2~10pg per injection for all components. The effects of age and sex of rat on the contents of the catecholamines and their metabolites in rat brain striatum were studied. The levels of DA and 5-HT contents of the 7 week old female rats were higher than those of the 7 week old male rats. As the age of rat increases, the contents of DOPAC increased significantly.

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Amperometric Determination of Anthracycline Antibiotics with the Mercury Film Thin Layer Flow Cell (수은피막 박막흐름전지를 이용한 Anthracycline계 항생제의 전류법 정량)

  • Kim, Kyung Eun;Hahn, Younghee
    • Analytical Science and Technology
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    • v.17 no.6
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    • pp.470-475
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    • 2004
  • The mercury film thin layer flow cell (MFTLFC) which yielded the highest sensitivity for the electrochemical reduction of doxorubicin was constructed by coating the glassy carbon working electrode (GCE; $A=0.208cm^2$) with $5{\mu}L$ of HgO coating solution (0.5% HgO + 0.25% polystyrene/cyclohexanone) and subsequently followed by applying a potential of -0.40 V for 300 sec in the flow stream of an acetate buffer of pH 4.5. The voltammogram of doxorubicin reached the diffusion current plateau at -0.53 V vs. a Ag/AgCl (3 M NaCl) in the MFTLFC. The diffusion current (Id) of doxorubicin at the MFTLFC was 1.7 times greater than the Id obtained at the TLFC employing a bare glassy carbon working electrode. When the peak areas (electric charge) were plotted vs. concentrations of standard anthracyclines, the calibration factors of doxorubicin and daunorubicin were $1.12{\times}10^8{\mu}C/M$ (coefficient of determination; $R^2$: 0.969) and $0.98{\times}10^8{\mu}C/M$> ($R^2$: 0.999), respectively in the concentration range between $1.0{\times}10^{-8}M$ and $1.0{\times}10^{-6}M$.

Detection of Urinary 8-Hydroxyguanine Adduct as Exposure Biomarker for Oxidative Stress (산화적스트레스에 대한 노출척도로서 뇨중 8-Hydroxyguanine Adduct의 측정)

  • 유아선;김윤신;모인필;마응천;조명행
    • Toxicological Research
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    • v.14 no.4
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    • pp.515-523
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    • 1998
  • Oxidative stress by reactive oxygen species (ROS) damages cellular DNA, RNA, proteins, lipids and others causing various diseases such as cancer, arthritis, and heart diseases. 8-Hydroxyguanine (8-OHG) is one of the products formed from DNA or RNA damaged by ROS. Since high amounts of 8-OHG can be excreted in urine, it may serve as a potential biomarker indicating the level of oxidative damage to nucleic acids. Residents in industrial area with severe air pollution are expected to be affected by higher level of oxidative stress from pollutants like polyaromatic hydrocarbons (PAHs), etc. Smokers are also expected to be damaged by higher level of oxidative stress from cigarette smoke components like PAHs than non-smokers. To examine if the determination of the urinary concentration of 8-OHG could be used as exposure biomarker for the oxidative stress caused by air-pollutants, this study was performed to determine and compare the urinary concentrations of 8-OHG in smokers and non-smokers, or non-polluted area residents and polluted area residents. Urine samples were collected and purified by a strong cation exchange and cellulose partition column, then analyzed by HPLC with electrochemical detector at 600 ㎷ potential. Concentrations of urinary 8-OHG in non-smokers and smokers of Seoul area college male students were determined as 15.12$\pm$9.68 (ng/mg creatinine) and 34.72$\pm$11.72 (ng/mg creatinine), respectively, showing significantly higher level of 8-OHG in smokers than in non-smokers. Urine samples of elementary school students were collected from Sokcho area, which is known to be non-polluted, and 3 representative polluted areas; Yocheon industrial area, Ulsan urban and Ulsan industrial area. The concentrations of 8-OHG in these samples were 12.42$\pm$8.27 (ng/ mg creatinine, Sokcho), 22.55$\pm$9.12 (ng/mg creatinine, Yocheon), 17.41$\pm$2.30 (ng/mg creatinine, Ulsan urban), 55.04$\pm$39.73 (ng/mg creatinine, Ulsan industrial). Thus, samples from polluted area tend to have higher level of 8-OHG and the levels of Yocheon and Ulsan industrial area were significantly higher than that of Sokcho area. The results indicate that the residents of polluted industrial area or smokers are more severely exposed to oxidative stress probably caused by air pollutants like PAHs. Thus, the determination of urinary 8-OHG concentration could be used as biomarker for the extent of body exposure to oxidative stress caused by various pollutants.

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Study on Electrode Selection for Electrochemical Detection of Cadmium and Lead (카드뮴과 납 전기화학적 검출을 위한 전극선정에 관한 연구)

  • Kim, Hak-Jin;Kim, Ki-Young;Moh, Chang-Yeon;Cho, Han-Keun
    • Journal of Biosystems Engineering
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    • v.33 no.6
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    • pp.404-409
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    • 2008
  • Excessive presence of heavy metals in environment affects plants and fruits grown in the contaminated area. Rapid on-site monitoring of heavy metals can provide useful information for efficiently characterizing heavy metal-contaminated sites and for minimizing the exposure of the contaminated food crops to humans. This study reports on the evaluation of gold and glassy carbon (GC) electrodes with mercury or bismuth as a coating material for simultaneous determination of cadmium (Cd) and lead (Pb) in 0.1 M $HNO_3$ solution by anodic stripping voltammetry (ASV). The use of a square-wave voltammetric potential between a working electrode and a reference electrode caused Cd and Pb ions deposited on the electrode surface to be oxidized, thereby generating electric currents at different potentials. The mercury-coated gold electrode was not sensitive enough to detect the usable range of Cd concentrations (1 to 100 ppb). The GC electrodes with mercury or bismuth displayed well-defined, sharp and separate current peaks for Cd and Pb ions when the square-wave voltammetric potentials were applied. The peak currents measured with both mercury- and bismuth- coated GC electrodes were linearly proportional to Cd and Pb concentrations in the range of 1 to 200 ppb in 0.1 M $HNO_3$ with strong linear relationships between concentration and peak current ($R^2$ > 0.95), indicating that both of Cd and Pb ions could be quantitatively measured.

Development of Electro-Biosensor for the Residual Pesticides using Organic Carbon and Cobalt Phthalocyanine (Cobalt Phthalocyanine 탄소유기 전극을 이용한 농약 잔류량 측정 센서개발)

  • Yu, Young-Hun;Cho, Hyung-Jun;Park, Won-Pyo;Hyun, Hae-Nam
    • Korean Journal of Environmental Agriculture
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    • v.29 no.1
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    • pp.72-76
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    • 2010
  • We have developed the bio-electrode measuring the variance of the amount of acetylcholine affected by residual pesticide. The working electrode of the biosensor was made by combination of cobalt phthalocyanine and carbon organic compounds. The biosensors were constructed by screen-printing method. The principle of working electrode is similar to thiocholine sensor. We have fabricated the biosensor using standard screen printing method. Generally, the biosensor made by printing method formed thick film biosensor. When the electrodes were made by electrochemical cells, the generation of current by the addition of enzyme substrate was inhibited by standard solutions of organo-phosphate pesticides. The detection limit of sensor is about 0.5 $\mu{g}/L$ for carbofuran. We could improve the responsibility of the sensor by controlling the cobalt phthalocyanine and thiocholine concentration ratio. Also we have tested the EPN and Chlorpyrifos pesticides and found that the biosensor is applicable to fast determination of residual pesticides.

Full Parametric Impedance Analysis of Photoelectrochemical Cells: Case of a TiO2 Photoanode

  • Nguyen, Hung Tai;Tran, Thi Lan;Nguyen, Dang Thanh;Shin, Eui-Chol;Kang, Soon-Hyung;Lee, Jong-Sook
    • Journal of the Korean Ceramic Society
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    • v.55 no.3
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    • pp.244-260
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    • 2018
  • Issues in the electrical characterization of semiconducting photoanodes in a photoelectrochemical (PEC) cell, such as the cell geometry dependence, scan rate dependence in DC measurements, and the frequency dependence in AC measurements, are addressed, using the example of a $TiO_2$ photoanode. Contrary to conventional constant phase element (CPE) modeling, the capacitive behavior associated with Mott-Schottky (MS) response was successfully modeled by a Havriliak-Negami (HN) capacitance function-which allowed the determination of frequency-independent Schottky capacitance parameters to be explained by a trapping mechanism. Additional polarization can be successfully described by the parallel connection of a Bisquert transmission line (TL) model for the diffusion-recombination process in the nanostructured $TiO_2$ electrode. Instead of shunt CPEs generally employed for the non-ideal TL feature, TL models with ideal shunt capacitors can describe the experimental data in the presence of an infinite-length Warburg element as internal interfacial impedance - a characteristic suggested to be a generic feature of many electrochemical cells. Fully parametrized impedance spectra finally allow in-depth physicochemical interpretations.

Review on the Determination of Frumkin, Langmuir, and Temkin Adsorption Isotherms at Electrode/Solution Interfaces Using the Phase-Shift Method and Correlation Constants

  • Chun, Jinyoung;Chun, Jang H.
    • Korean Chemical Engineering Research
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    • v.54 no.6
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    • pp.734-745
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    • 2016
  • This review article described the electrochemical Frumkin, Langmuir, and Temkin adsorption isotherms of over-potentially deposited hydrogen (OPD H) and deuterium (OPD D) for the cathodic $H_2$ and $D_2$ evolution reactions (HER, DER) at Pt, Ir, Pt-Ir alloy, Pd, Au, and Re/normal ($H_2O$) and heavy water ($D_2O$) solution interfaces. The Frumkin, Langmuir, and Temkin adsorption isotherms of intermediates (OPD H, OPD D, etc.) for sequential reactions (HER, DER, etc.) at electrode/solution interfaces are determined using the phase-shift method and correlation constants, which have been suggested and developed by Chun et al. The basic procedure of the phase-shift method, the Frumkin, Langmuir, and Temkin adsorption isotherms of OPD H and OPD D and related electrode kinetic and thermodynamic parameters, i.e., the fractional surface coverage ($0{\leq}{\theta}{\leq}1$) vs. potential (E) behavior (${\theta}$ vs. E), equilibrium constant (K), interaction parameter (g), standard Gibbs energy (${\Delta}G_{\theta}{^{\circ}}$) of adsorption, and rate (r) of change of ${\Delta}G_{\theta}{^{\circ}}$ with ${\theta}$ ($0{\leq}{\theta}{\leq}1$), at the interfaces are briefly interpreted and summarized. The phase-shift method and correlation constants are useful and effective techniques to determine the Frumkin, Langmuir, and Temkin adsorption isotherms and related electrode kinetic and thermodynamic parameters (${\theta}$ vs. E, K, g, ${\Delta}G_{\theta}{^{\circ}}$, r) at electrode/solution interfaces.

Development of HRP-modified Carbon Composite Biosensor and Electrochemical Analysis of H2O2 (Horseradish peroxidase가 변성된 탄소복합 바이오센서 개발 및 전기화학적 H2O2분석)

  • Park, Deog-Su
    • Journal of the Korean Chemical Society
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    • v.56 no.5
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    • pp.571-576
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    • 2012
  • A sol-gel derived carbon composite electrodes (CCEs) were fabricated by mixing horseradish peroxidase (HRP), sol of tetraethoxysilane (TESO), and graphite powder. The HRP solution was added to the sol solution of TEOS, and then graphite powder was added to this mixture. The resulting carbon ceramic network effectively encapsulated HRP and shows a catalytic reduction starting at -0.2 V for $H_2O_2$. The optimum conditions for $H_2O_2$determination have been characterized with respect to the enzyme loading ratio and pH. The linear range and detection limit of $H_2O_2$ detection were from 0.2 mM to 2.2 mM and 0.035 mM, respectively. The common electroactive interferences such as ascorbic acid, acetaminophene, and uric acid were not affected upon the response to $H_2O_2$ at the HRP biosensor due to low detection potential.

Optimization of Analytical Procedure for Hydrogen Cyanide in Mainstream Smoke

  • Lee, John-Tae;Kim, Hyo-Keun;Hwang, Keon-Joong;Jang, Gi-Chul;Lee, Jeong-Min;Kim, Ick-Joong
    • Journal of the Korean Society of Tobacco Science
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    • v.29 no.2
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    • pp.125-131
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    • 2007
  • Hydrogen cyanide(HCN), formed from pyrolysis of various nitrogenous compounds such as protein, amino acids and nitrate in tobacco, is present in both the particulate phase and vapor phase of cigarette smoke. Typically the determination of HCN in cigarette smoke has been done through colorimetric and electrochemical techniques, such as fluorescence spectrometry, UV-spectrophotometry (UV), continuous flow analyzer (CFA), capillary GC-ECD and ion chromatography (IC). Most of these techniques are known to be time-consuming and some of them lack specificity or sensitivity. The available results from both our laboratory and reported literatures for 2R4F Kentucky reference cigarette, smoked under ISO condition, show a relatively wide variation ranging from 100 to 120 ug/cig of HCN. Especially, the precision and accuracy of the analytical results of HCN tend to get worse in low tar cigarettes and under intense smoking condition. In this paper, a more optimized analytical methods than previous ones are suggested. This method shows lower detection limit and has improved precision and accuracy, so it is applicable for wide tar level cigarettes under intense smoking condition as well as under ISO smoking condition. Important features of this method are improved sample collection and quantification systems such as the number of trapping units, volume, temperature and type of trapping solution. To avoid volatilization loss of HCN in analyzing mainstream smoke, it is highly recommended that pH values of trapping solutions should be maintained over 11 and cold traps should be used in collecting mainstream smoke.

Influence of Current Density Application Time on the Corrosion Damage of Offshore Wind Steel Substructure in Galvanostatic Corrosion Experiment (해상풍력 하부 구조물용 강재의 정전류 부식 시험 시 전류밀도 인가 시간이 부식손상에 미치는 영향)

  • Lee, Jung-Hyung;Park, Jae-Cheul;Han, Min-Su;Jang, Seok-Ki;Kim, Seong-Jong
    • Journal of Surface Science and Engineering
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    • v.49 no.5
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    • pp.431-438
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    • 2016
  • This research investigated the relationship between the corrosion damage characteristics of offshore wind steel substructure and the time of current density application by electrochemical accelerated short-term corrosion test. The galvanostatic corrosion was conducted on the steel specimens in natural seawater with a constant current density ranging from $1mA/cm^2$ to $200mA/cm^2$ for 1 ~ 180 min. Macro and micro observation was carried out on the surface of the corrosion damaged area using SEM and 3-dimensional analysis microscope. The weight loss of the specimens before and after was calculated as the difference between the initial weight prior to corrosion and weight after removal of the corrosion product. It was shown that during galvanostaic corrosion process, the corrosion behavior could be characterized by the onset of pitting corrosion in the early stage and the uniform corrosion in the late stage, showing damage development in the depth direction with the time of current application. The result of the 3D analysis revealed that both damage depth and surface roughness increased with increasing time of current application. The weight loss curves with time showed that a coefficient of determination ($R^2$) was relatively high for the relationship between the time of current application and weight loss. As a result, the degree of corrosion can be controlled by simply varying the time of current application.